CN114921108B - Modified asphalt and preparation method thereof - Google Patents
Modified asphalt and preparation method thereof Download PDFInfo
- Publication number
- CN114921108B CN114921108B CN202210791060.4A CN202210791060A CN114921108B CN 114921108 B CN114921108 B CN 114921108B CN 202210791060 A CN202210791060 A CN 202210791060A CN 114921108 B CN114921108 B CN 114921108B
- Authority
- CN
- China
- Prior art keywords
- asphalt
- temperature
- shearing
- matrix
- zinc oxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/201—Pre-melted polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/12—Esters; Ether-esters of cyclic polycarboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/521—Esters of phosphoric acids, e.g. of H3PO4
- C08K5/523—Esters of phosphoric acids, e.g. of H3PO4 with hydroxyaryl compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2395/00—Bituminous materials, e.g. asphalt, tar or pitch
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/329—Phosphorus containing acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A30/00—Adapting or protecting infrastructure or their operation
- Y02A30/60—Planning or developing urban green infrastructure
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a modified asphalt and a preparation method thereof, and raw materials comprise base asphalt, nano zinc oxide, polyphosphoric acid and a plasticizer, wherein the doping amount of the nano zinc oxide is 0.5-1.5% of the mass of the base asphalt, the doping amount of the polyphosphoric acid is 0.5-1.1% of the mass of the base asphalt, and the doping amount of the plasticizer is 1-2% of the mass of the base asphalt. The modified asphalt provided by the invention has good high-temperature performance, temperature sensitivity, low-temperature performance and thermal stability, greatly improves the ageing resistance and fatigue resistance, is not easy to separate and segregate, and is convenient for long-term storage.
Description
Technical Field
The invention belongs to the technical field of road engineering materials, relates to modified asphalt and a preparation method thereof, and particularly relates to nano material/polymer modified asphalt and a preparation method thereof.
Background
In recent years, a modifier material for asphalt is diversified in the technical field of road engineering materials, polyphosphoric acid (PPA) can react with matrix asphalt chemically, the modification process is simple, the price is low, the using amount is small, the temperature sensitivity of an asphalt mixture can be obviously improved, and the adaptability of an asphalt road to heavy traffic is improved, so that the PPA is selected to replace the traditional polymer modifier. After PPA is added into the base asphalt, the chemical structure of the asphalt is changed, and hydroxyl in the PPA chemical structure reacts with polar groups in the asphalt to generate ether or ester. Cyclization and grafting occur among carbon chains, so that the molecular structure of the asphalt is more complex, and the high-temperature performance of the asphalt is improved. The PPA modified asphalt has obviously improved high-temperature anti-rutting capability, increased elastic modulus and reduced phase angle, and the 1 percent PPA and 4 percent SBS have equivalent capability of improving the high-temperature stability of the asphalt. The PPA is compounded with SBS modifier, SBR modifier, rubber powder, etc. to form asphalt modifier, and the asphalt modifier is used in raising the high temperature performance of composite modified asphalt. However, PPA has a large influence on the low-temperature performance of the asphalt, so that the low-temperature performance of the asphalt is obviously reduced, and the aging resistance of the PPA modified asphalt in a long-term aging mode is poor.
Disclosure of Invention
In order to solve the problems, the invention provides modified asphalt which has good high-temperature performance, temperature sensitivity, low-temperature performance and thermal stability, greatly improves the anti-aging capability and fatigue resistance, is not easy to separate and segregate, is convenient for long-term storage, and solves the problems in the prior art.
Another object of the present invention is to provide a process for producing a modified asphalt.
The technical scheme adopted by the invention is that the modified asphalt comprises the raw materials of matrix asphalt, nano zinc oxide, polyphosphoric acid and a plasticizer, wherein the doping amount of the nano zinc oxide is 0.5-1.5% of the mass of the matrix asphalt, the doping amount of the polyphosphoric acid is 0.5-1.1% of the mass of the matrix asphalt, and the doping amount of the plasticizer is 1-2% of the mass of the matrix asphalt.
Further, the specific surface area of the nano zinc oxide is 50-55m 2 Per g, average grain diameter of 30 +/-1 nm and purity of more than 99.5 percent.
Further, the plasticizer is any one of dioctyl phthalate, dibutyl phthalate, tricresyl phosphate, triphenyl phosphate and dioctyl sebacate.
The preparation method of the modified asphalt comprises the following steps:
s1, heating and drying matrix asphalt and enough nano zinc oxide at 130-135 ℃ respectively to enable the matrix asphalt to have better fluidity; drying the water in the nano zinc oxide;
s2, taking out the matrix asphalt, uniformly heating to 145-150 ℃, and adding nano zinc oxide into the matrix asphalt, wherein the doping amount of the nano zinc oxide is 0.5-1.5% of the mass of the matrix asphalt; stirring uniformly, and shearing at high speed;
s3, adding polyphosphoric acid, wherein the mixing amount of polyphosphoric acid is 0.5-1.1% of the mass of the matrix asphalt, uniformly stirring, and shearing at a high speed;
s4, adding a plasticizer in a ratio of 1% -2% of the matrix asphalt, uniformly stirring, and shearing at a high speed;
and S5, putting the sheared modified asphalt into an oven at the temperature of 145-150 ℃ for development to obtain the modified asphalt.
Further, in the step S1, the heating and drying time is 1 to 1.5 hours.
Further, in step S2, the uniformly heating specifically includes: and (2) putting the matrix asphalt heated in the step (S1) into a heat collection pot of a magnetic stirrer for oil bath heating, keeping the temperature at 145-150 ℃, starting a shearing machine, and stirring the matrix asphalt at the speed of 500-800r/min to uniformly heat the matrix asphalt until the internal temperature of the matrix asphalt is stable.
Further, in the steps S2 and S3, the shearing speed of high-speed shearing is 3000-3500r/min, the shearing temperature is 145-150 ℃, and the shearing time is 10-15min.
Further, in the step S4, the shearing speed of high-speed shearing is 3000-3500r/min, the shearing temperature is 145-150 ℃, and the shearing time is 20-30min.
Further, in the step S4, the plasticizer is any one of dioctyl phthalate, dibutyl phthalate, tricresyl phosphate, triphenyl phosphate, or dioctyl sebacate.
Further, the development time in the oven in the step S5 is 40-60min.
The invention has the beneficial effects that:
1. according to the invention, a nano zinc oxide material, polyphosphoric acid (PPA) and a plasticizer (DOP) are selected to carry out composite modification on the matrix asphalt, and the nano zinc oxide is utilized to enhance the diffusion capacity of the polyphosphoric acid in the matrix asphalt, so that the cyclization and grafting reaction between the polyphosphoric acid and the asphalt component are more sufficient; compared with the method of singly using polyphosphoric acid as the modifier of the modified asphalt, the method can further improve the high-temperature performance and the temperature sensitivity of the matrix asphalt and further enhance the rutting resistance of the polyphosphoric acid modified asphalt in high-temperature areas.
2. The invention improves the storage stability of the modified asphalt by the surface effect, small-size effect, quantum size effect and macroscopic quantum tunneling effect of the nano zinc oxide particles, compared with SBS modified asphalt, the high-performance nano/polymer modified asphalt prepared by the invention is not easy to separate and isolate in layers, so that the modified asphalt product can be stored for a long time and can be taken at any time, the mixing amount of the modifier is low, the phenomenon of pipeline blockage in the pumping process can not occur in the engineering use, and the engineering usability of the modified asphalt is improved.
3. The nano ZnO and the plasticizer can be uniformly dispersed in the matrix asphalt and can generate a cross-linking reaction with the asphalt to generate a space network structure, so that the low-temperature performance and the thermal stability of the polyphosphoric acid (PPA) modified asphalt are effectively improved at the same time. The nano ZnO particles have a certain reflection effect on ultraviolet rays, the basic performance of the nano ZnO particles is improved more obviously after surface modification, and the nano ZnO particles show excellent ultraviolet aging resistance, and the modified asphalt compounded with polyphosphoric acid (PPA) and a plasticizer can greatly improve the comprehensive aging resistance of the modified asphalt, effectively improve the thermal oxidation resistance of the modified asphalt under natural conditions and the aging resistance of natural ultraviolet rays on the asphalt, improve the fatigue resistance of the asphalt and prolong the service life of roads.
4. The plasticizer can greatly improve the sliding capacity among internal molecules of the asphalt and between asphalt molecules and the modifier, increase the free volume of the modified asphalt, enhance the moving capacity of the modifier among the matrix asphalt, and greatly improve the low-temperature performance of the composite modified asphalt while not remarkably reducing the high-temperature performance of the nano zinc oxide and PPA composite modified asphalt.
5. The preparation method has simple process, can be completed only by common shearing and stirring equipment or a circulating system, has less investment requirements on capital construction, equipment and the like for producing the modified asphalt, and has wider application range. Compared with the traditional SBS modified asphalt, the preparation temperature is reduced by 25-30%, the preparation time is shorter, the energy consumption is less, the influence on the asphalt aging in the preparation process is less, and the polyphosphoric acid (PPA) is low in price, has a certain cost advantage, and is more favorable for large-scale industrial production.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the prior art descriptions will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 shows the influence of nano zinc oxide on three major indexes of matrix asphalt in the embodiment of the invention.
FIG. 2 shows the effect of PPA on three major indicators of asphalt matrix in an example of the present invention.
FIG. 3 shows the effect of the plasticizer DOP on three major indicators of asphalt in the examples of the present invention.
FIG. 4 shows the change of storage modulus G'/Pa at 64 ℃ with frequency of the modified asphalt prepared by the example of the present invention.
FIG. 5 is a graph showing the 64 ℃ loss modulus G'/Pa as a function of frequency for modified asphalt prepared according to an example of the present invention.
FIG. 6 is the creep stiffness of modified asphalt prepared by examples of the present invention.
FIG. 7 is a graph showing the creep rate of modified asphalt prepared by examples of the present invention.
FIG. 8 is the AI index after long-term aging of the modified asphalt prepared by the example of the present invention.
FIG. 9 is the RAI index after long term aging of the modified asphalt prepared by the examples of the present invention.
FIG. 10 is the SAI index after UV aging of modified asphalt made in accordance with an embodiment of the present invention.
FIG. 11 shows the mAI index after UV aging of the modified asphalt made in accordance with the example of the invention.
FIG. 12 is a comparison of penetration of the composite modified asphalts of examples 6 and 7 of the present invention.
FIG. 13 is a comparison of the softening points of the modified asphalt compositions obtained in examples 6 and 7 of the present invention.
FIG. 14 is a comparison of ductility of composite modified asphalt obtained in examples 6 and 7 of the present invention.
FIG. 15 is a scanning electron microscope (50 μm) of nano zinc oxide-modified asphalt (JN).
FIG. 16 is a scanning electron micrograph (50 μm) of PPA-modified asphalt (JP).
FIG. 17 is a scanning electron micrograph (50 μm) of composite modified asphalt (JC) according to an example of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the case of the example 1, the following examples are given,
the modified asphalt comprises the raw materials of nano zinc oxide, polyphosphoric acid and a plasticizer, wherein the dosage of the nano zinc oxide is 0.5-1.5 percent of the weight of the matrix asphalt, the dosage of PPA (polyphthalate) is 0.5-1.1 percent of the weight of the matrix asphalt, and the dosage of DOP is 1-2 percent of the weight of the matrix asphalt.
In the case of the example 2, the following examples are given,
the preparation method of the modified asphalt comprises the following steps:
s1, respectively putting the matrix asphalt and enough nano-zinc oxide into an oven at 130-135 ℃, heating for 1-1.5 hours to ensure that the matrix asphalt has better fluidity, and drying the water in the nano-zinc oxide to keep the nano-zinc oxide dry. The nano zinc oxide is dried mainly because the specific surface area of the nano material is large, water vapor is easily absorbed under natural conditions, and the purpose of drying is to remove water possibly existing in the modifier and avoid the influence of the water on the asphalt modification effect.
S2, taking out the matrix asphalt, putting the matrix asphalt into a heat collection pot of a magnetic stirrer (DF-101T-5) for oil bath heating, and keeping the temperature at 145-150 ℃. The matrix asphalt is petroleum asphalt No. 70, and the related parameters of the nano zinc oxide are shown in the following table 1.
TABLE 1 parameters associated with the nano-zinc oxide
| Item | Index (I) |
| Specific surface area | 50-55m 2 /g |
| |
30±1nm |
| Purity of | ＞99.5％ |
Starting a high-speed shearing machine (GS-1 type), and stirring the matrix asphalt at a speed of 500-800r/min to ensure that the matrix asphalt is uniformly heated. After the internal temperature of the matrix asphalt is stable, adding the nano zinc oxide into the matrix asphalt according to a proportion, stirring by using a glass rod, adjusting the rotating speed to 3000-3500r/min, and shearing for 10-15 minutes at the shearing temperature of 145-150 ℃. The dosage of the nano zinc oxide is 0.5 to 1.5 percent of the weight of the matrix asphalt.
And S3, continuously adding polyphosphoric acid (PPA) according to the proportion, wherein the dosage of PPA is 0.5-1.1 percent of the weight of the matrix asphalt, stirring by using a glass rod, keeping the temperature at 145-150 ℃, rotating speed at 3500r/min, and shearing for 10-15 minutes. The related parameters of the PPA material are shown in Table 2, and the molecular formula is as follows:
TABLE 2 PPA-related parameters
| Item | Index (I) |
| Phosphorus pentoxide (%) | ≥80 |
| Heavy metals (in terms of Pb) (%) | ≤0.01 |
| Insoluble (%) | ≤0.02 |
| Iron (%) | ≤0.01 |
| Sulfate (%) | ≤0.02 |
| Specific gravity (g/cm) 3 ) | ≥2.1 |
S4, adding a plasticizer in proportion, wherein the plasticizer is any one of dioctyl phthalate (DOP), dibutyl phthalate (DBP), tricresyl phosphate, triphenyl phosphate and dioctyl sebacate; the mixing amount is 1-2% of the mass of the matrix asphalt, the mixture is stirred by a glass rod after being added, the temperature is continuously kept at 145-150 ℃, the rotating speed is 3000-3500r/min, and the mixture is sheared for 20-30min. The plasticizer is a viscous liquid with high boiling point and difficult volatilization or a solid with low melting point, and dioctyl phthalate (DOP) can reduce the hardness and the catalytic temperature of the material, effectively improve the low-temperature performance of the asphalt, but has certain adverse effect on the high-temperature performance.
In the steps S2-S4, the glass rod is used for stirring, so that the three modifiers are dispersed, the modifiers are prevented from floating on the surface of the asphalt, the modifiers and the asphalt cannot be sufficiently sheared and mixed, and the modification effect is reduced.
In the steps S2-S4, the shearing temperature refers to the temperature of the modified asphalt measured by a thermometer in the shearing process, but not the temperature of the oil bath; the purpose of controlling the shearing temperature to 145-150 ℃ is to reduce the influence of asphalt aging on the performance of the modified asphalt in the shearing process, ensure the modification effect and reduce the energy consumption. The high temperature can cause the segregation phenomenon of the asphalt modifier and accelerate the volatilization of light components in the base asphalt and the thermal-oxidative aging of the base asphalt. The excessively low temperature can cause the viscosity of the asphalt to be excessively high, so that the shearing resistance is excessively high, the modifier can not be fully sheared and uniformly dispersed, and the modification effect is reduced.
And S5, putting the sheared modified asphalt into an oven with the temperature of 145-150 ℃ for development for 40-60min to obtain the high-performance nano/polymer modified asphalt. The main development purpose is to eliminate air bubbles possibly generated in the modified asphalt in the shearing process, avoid the influence of the air bubbles on the subsequent experimental processes such as mold casting and the like, and fully enable the modifier to generate chemical reaction with the matrix asphalt under the static action to exert the modification effect. The development temperature of the oven and the shearing temperature are kept consistent mainly because the modified asphalt is easy to generate the phenomenon of layering and segregation and is easy to age due to overhigh temperature. The excessively low temperature can reduce the surface temperature of the asphalt, so that the temperature difference is generated inside and outside the modified asphalt, the overflow of internal bubbles is not facilitated, the reaction rate of the modifier and the asphalt is reduced, and the modification effect is reduced.
In the case of the example 3, the following examples are given,
a preparation method of modified asphalt specifically comprises the following steps:
s1, respectively heating and drying matrix asphalt and enough nano zinc oxide in a drying oven at 130 ℃ for 1 hour to ensure that the matrix asphalt has better fluidity; and drying the water in the nano zinc oxide to keep the nano zinc oxide dry.
S2, taking out the matrix asphalt, putting the matrix asphalt into a heat collection pot of a magnetic stirrer for oil bath heating, keeping the temperature at 145 ℃, starting a shearing machine, and stirring the matrix asphalt at the speed of 500r/min to ensure that the matrix asphalt is uniformly heated until the internal temperature of the matrix asphalt is stable; adding nano zinc oxide into the matrix asphalt, wherein the doping amount of the nano zinc oxide is 0.5 percent of the mass of the matrix asphalt; stirring uniformly, wherein the shearing speed is 3000r/min, the shearing temperature is 145 ℃, and the shearing time is 10min.
And S3, adding polyphosphoric acid, wherein the mixing amount of polyphosphoric acid is 1.1 percent of the mass of the matrix asphalt, uniformly stirring, and shearing at the speed of 3000r/min and the temperature of 145 ℃ for 10min.
And S4, adding dibutyl phthalate (DBP) in proportion, wherein the mixing amount is 1% of that of the matrix asphalt, uniformly stirring, and shearing at the speed of 3000r/min and the temperature of 145 ℃ for 20min.
And S5, putting the sheared modified asphalt into an oven with the temperature of 145 ℃ for development for 60min to obtain the modified asphalt.
In the case of the example 4, it is preferred,
a preparation method of modified asphalt specifically comprises the following steps:
s1, respectively heating and drying matrix asphalt and enough nano zinc oxide in a 135 ℃ oven for 1.5 hours to ensure that the matrix asphalt has better fluidity; and drying the water in the nano zinc oxide to keep the nano zinc oxide dry.
S2, taking out the matrix asphalt, putting the matrix asphalt into a heat collection pot of a magnetic stirrer for oil bath heating, keeping the temperature at 150 ℃, starting a shearing machine, and stirring the matrix asphalt at a speed of 800r/min to ensure that the matrix asphalt is uniformly heated until the internal temperature of the matrix asphalt is stable; adding nano zinc oxide into the matrix asphalt, wherein the doping amount of the nano zinc oxide is 1.5 percent of the mass of the matrix asphalt; stirring uniformly, wherein the shearing speed is 3500r/min, the shearing temperature is 150 ℃, and the shearing time is 15min.
And S3, adding polyphosphoric acid, wherein the mixing amount of polyphosphoric acid is 0.5 percent of the mass of the matrix asphalt, uniformly stirring, and shearing at the temperature of 150 ℃ for 10min at the shearing speed of 3500 r/min.
S4, adding tricresyl phosphate according to the proportion, wherein the mixing amount is 1 percent of that of the matrix asphalt, uniformly stirring, and shearing at the speed of 3500r/min and the temperature of 150 ℃ for 30min.
And S5, putting the sheared modified asphalt into an oven with the temperature of 150 ℃ for development for 40min to obtain the modified asphalt.
In the case of the example 5, the following examples were conducted,
the preparation method of the modified asphalt comprises the following steps:
s1, respectively heating and drying matrix asphalt and enough nano zinc oxide in an oven at 132 ℃ for 1.2 hours to ensure that the matrix asphalt has better fluidity; and drying the water in the nano zinc oxide to keep the nano zinc oxide dry.
S2, taking out the matrix asphalt, putting the matrix asphalt into a heat collection pot of a magnetic stirrer for oil bath heating, keeping the temperature at 140 ℃, starting a shearing machine, and stirring the matrix asphalt at the speed of 700r/min to ensure that the matrix asphalt is uniformly heated until the internal temperature of the matrix asphalt is stable; adding nano zinc oxide into the matrix asphalt, wherein the doping amount of the nano zinc oxide is 1 percent of the mass of the matrix asphalt; stirring uniformly, wherein the shearing speed is 3200r/min, the shearing temperature is 148 ℃, and the shearing time is 12min.
And S3, adding polyphosphoric acid, wherein the mixing amount of polyphosphoric acid is 0.8 percent of the mass of the matrix asphalt, uniformly stirring, and shearing at the shearing speed of 3200r/min and the shearing temperature of 148 ℃ for 12min.
And S4, adding triphenyl phosphate according to a proportion, wherein the mixing amount is 1.5 percent of that of the matrix asphalt, uniformly stirring, and shearing at a shearing speed of 3200r/min and a shearing temperature of 148 ℃ for 25min.
And S5, putting the sheared modified asphalt into an oven with the temperature of 148 ℃ to grow for 50min to obtain the asphalt.
The temperatures of the steps S2 to S5 of the invention are not necessarily required to be completely consistent, the lower limit of the temperature is to ensure that the asphalt is in a flowing state, and the upper limit of the temperature is to control the upper limit of the temperature so as to obtain a corresponding product at a lower temperature, reduce energy consumption and reduce the volatilization loss of light components caused by high-temperature preparation. The temperature in S5 represents the development temperature, and mainly volatilizes bubbles in the asphalt in a flowing state to reduce the influence on the experiment.
After the doping amount of the nano zinc oxide exceeds 1.5%, the effects of reducing the penetration degree and improving the softening point of the base asphalt are not obvious, namely the improvement degree of the high-temperature effect is reduced, but the ductility of the base asphalt at 5 ℃ is reduced, and the low-temperature effect is worse and worse, as shown in figure 1. When the amount of the nano zinc oxide reaches a certain degree, the modified asphalt has obvious modification effect, and the amount of the nano zinc oxide is too small to be sufficiently distributed in the matrix asphalt, so that no nano zinc oxide is locally used for performing the modification effect, and the effect is not obvious.
The specific surface area of the nano zinc oxide is too large or the average particle size is too small, so that the nano zinc oxide is not easy to disperse in asphalt, an agglomeration phenomenon is formed, and the modification effect is reduced. Too small specific surface area or too large average particle size can result in poor compatibility of zinc oxide and asphalt, easily cause segregation phenomenon, and affect storage stability of the modified asphalt. The purity of the nano zinc oxide refers to the effective component of the nano zinc oxide in the modifier, the purity is more than 99.5%, and if the purity is too low and does not meet the index, more impurities are mixed into the modified asphalt to influence the composite modification effect.
The nanometer material as a novel modifier can change the asphalt structure microscopically, thereby improving the macroscopic property of the asphalt. The nano material is added into the asphalt, so that the high-temperature stability, the fatigue resistance, the skid resistance, the ageing resistance, the durability, the water stability and the like of the asphalt can be improved. The nano zinc oxide as one of the nano materials can fully perform chemical reaction with the substrate asphalt to form a stable asphalt system, and meanwhile, the metal oxide can effectively improve the ultraviolet aging resistance of the asphalt by reflecting natural light.
After the plasticizer is added into the traditional modified asphalt, although the fluidity of the asphalt at low temperature is greatly improved, the high-temperature performance of the asphalt is greatly damaged, and pavement diseases such as rutting and the like can be more easily generated when the asphalt is used in hot summer. The special effect of the embodiment of the invention is that after the nano zinc oxide and the polyphosphoric acid are doped, the nano zinc oxide and the polyphosphoric acid are wrapped by asphalt macromolecules and simultaneously generate chemical reaction with asphalt molecules to form a cross-linked graft structure, and when no plasticizer exists, the high-temperature performance of the asphalt is improved due to the effect of chemical bonds. After the plasticizer is added, the plasticizer is inserted into a three-dimensional network structure formed between the nano zinc oxide and the matrix asphalt, so that the fluidity of the asphalt can be increased, and the network structure formed by the nano zinc oxide and the asphalt can limit the free movement of molecules in the asphalt to a certain extent, so that the low-temperature performance of the asphalt can be improved, and the high-temperature performance of the asphalt can be improved by using the network structure of the nano zinc oxide.
In the examples, the PPA content is 0.5%, 0.8%, 1.1% by weight of the base asphalt, and when the PPA content exceeds 1.1%, although the penetration of the base asphalt is continuously reduced and the softening point of the base asphalt is increased, the ductility at 5 ℃ is excessively reduced, so that the brittleness of the asphalt is remarkably increased, and the low-temperature effect of the asphalt is severely reduced, as shown in fig. 2. When the PPA dosage reaches a certain degree, the modification effect of the modified asphalt is obvious, and the dosage is too small to be fully distributed in the matrix asphalt, so that the PPA does not play a modification role locally, and the effect is not obvious.
Phosphorus pentoxide is a main component in PPA for asphalt, so the content of the phosphorus pentoxide is not excessively low, and the modification effect is reduced due to the excessively low content of the phosphorus pentoxide. Substances such as heavy metals, insoluble substances, iron, sulfate and the like do not have good compatibility with asphalt and have negative influence on the modification effect, so the content of several substances in the modifier should be strictly limited.
In the embodiment of the invention, dioctyl phthalate (DOP) is adopted, the doping amount of the DOP is respectively 1%, 1.5% and 2% of the weight of the matrix asphalt, when the doping amount exceeds 2%, the light components of the matrix asphalt are too much, the viscosity is reduced, and the ductility at 5 ℃ is too high, so that the asphalt has too large plasticity, is easy to deform under high-temperature use, and has great influence on high-temperature performance. When the doping amount is less than 1%, the low-temperature improvement effect is not obvious, as shown in figure 3; therefore, the DOP content is selected to be 1%, 1.5% or 2%. The type of the plasticizer can be selected according to actual requirements, the environment-friendly requirement is high, plasticizers such as tributyl citrate and acetyl tributyl citrate can be selected, and the plasticizer is simple to synthesize and wide in source.
The lubricating effect of the plasticizer is not only simple lubrication among molecules, but also certain relative motion capability is provided among a three-dimensional network structure formed by the nano zinc oxide, the PPA and the asphalt and free asphalt molecules, so that the nano ZnO and the PPA improve the integral strength after part of matrix asphalt is integrated, and meanwhile, certain fluidity and flexibility are provided, so that the rheological property of the nano ZnO and the PPA at low temperature is improved, the phenomenon that cracks are generated due to cracking of a road surface caused by overlarge brittleness when the temperature is too low is avoided, and the fatigue resistance of the nano ZnO and the PPA is improved. Therefore, the plasticizer is added at last in the embodiment of the invention, so that the three-dimensional network structure is formed in the matrix asphalt firstly, and then the plasticizer is inserted into the three-dimensional network structure to provide the movement capability for the free asphalt molecules limited by the network structure, so that the composite modifier can improve the low-temperature cracking resistance of the asphalt while improving the high-temperature performance of the asphalt.
If the plasticizer is added firstly, the acting force between macromolecules in the matrix asphalt can be reduced, so that PPA and nano ZnO cannot be tightly combined with the matrix asphalt for reaction, the generated three-dimensional network structure is low in strength and loose in dispersion, and the high-temperature performance of the matrix asphalt is not obviously improved.
In the case of the example 6, it is preferred that,
a preparation method of modified asphalt (adding plasticizer DOP) specifically comprises the following steps:
s1, heating the matrix asphalt for 1-1.5 hours to ensure that the matrix asphalt has better fluidity, and removing water possibly existing in a modifier;
s2, taking out the matrix asphalt, putting the matrix asphalt into a heat collection pot of a magnetic stirrer (DF-101T-5) for oil bath heating, and keeping the temperature at 145-150 ℃. Starting a high-speed shearing machine (GS-1 type), and stirring the matrix asphalt at the speed of 500-800r/min to ensure that the matrix asphalt is uniformly heated; after the internal temperature of the matrix asphalt is stable, adding nano ZnO in a proportion with the amount of 1.5 percent of the weight of the matrix asphalt, stirring by a glass rod, keeping the temperature at 145-150 ℃ and the rotating speed at 3500r/min, and shearing for 10-15 minutes;
s3, adding PPA into the matrix asphalt according to a proportion, wherein the mixing amount is 0.5 percent of the mass of the matrix asphalt, stirring by using a glass rod, adjusting the rotating speed to 3000-3500r/min, and shearing for 10-15 minutes at the shearing temperature of 145-150 ℃;
s4, adding DOP according to the proportion, wherein the DOP accounts for 1.5 percent of the weight of the matrix asphalt, stirring by using a glass rod after adding, continuously keeping the temperature at 145-150 ℃, the rotating speed at 3000-3500r/min, and shearing for 20-30min;
and S5, putting the sheared modified asphalt into an oven with the temperature of 145-150 ℃ for development for 40-60min to obtain the modified asphalt.
In the case of the example 7, the following examples are given,
a preparation method of modified asphalt (adding plasticizer DOP) comprises the following steps:
s1, heating the base asphalt for 1-1.5 hours to ensure that the base asphalt has better fluidity and remove water possibly existing in the modifier.
S2, taking out the matrix asphalt, putting the matrix asphalt into a heat collection pot of a magnetic stirrer (DF-101T-5) for oil bath heating, and keeping the temperature at 145-150 ℃. Starting a high-speed shearing machine (GS-1 type), and stirring the matrix asphalt at the speed of 500-800r/min to ensure that the matrix asphalt is uniformly heated; after the internal temperature of the matrix asphalt is stable, adding DOP into the matrix asphalt according to a proportion, stirring by using a glass rod, adjusting the rotating speed to 3000-3500r/min, and shearing for 10-15 minutes at the shearing temperature of 145-150 ℃; the DOP dosage is 1.5 percent of the weight of the matrix asphalt;
s3, continuously adding nano ZnO according to the proportion, wherein the using amount of the nano ZnO is 1.5 percent of the weight of the matrix asphalt, stirring the mixture by using a glass rod, keeping the temperature at 145-150 ℃, the rotating speed at 3500r/min, and shearing the mixture for 10-15 minutes.
S4, PPA is added according to the proportion, the mixing amount is 0.5 percent of the mass of the matrix asphalt, the mixture is stirred by a glass rod after the PPA is added, the temperature is kept to be 145-150 ℃, the rotating speed is 3000-3500r/min, and the mixture is sheared for 20-30min.
And S5, putting the sheared modified asphalt into an oven with the temperature of 145-150 ℃ for development for 40-60min to obtain the modified asphalt.
The composite modified asphalt obtained in example 6 and example 7 were compared in three criteria, as shown in FIGS. 12 to 14.
By comparing the three indexes, it can be seen that the low-temperature ductility of the asphalt is not greatly different due to different charging sequences, but the penetration is improved and the softening point is reduced due to the fact that the plasticizer is added firstly compared with the penetration of the composite modified asphalt with the plasticizer added later, which indicates that the high-temperature performance of the composite modified asphalt is better than that of the modified asphalt with the plasticizer added firstly by adding the plasticizer later.
In the experimental example 1, the following experiments were carried out,
the SPSS software is used for carrying out range and variance analysis on orthogonal test results, and the influence degree of different mixing amounts of different modifiers on the basic physical properties of the composite modified asphalt is researched as shown in tables 3 to 6.
The doping of A (ZnO) is mainly used for improving the ultraviolet aging resistance of the asphalt, and the ductility index is increased with the increase of the doping amount of ZnO. Therefore, the A (ZnO) level is selected to be A3 in comprehensive consideration. B (PPA) mainly has a main influence on the ductility index, and the softening point is linearly increased along with the increase of the PPA doping amount, and the ductility is linearly reduced, so that the B (PPA) horizontal doping amount is selected as B1 by comprehensive consideration. C (DOP) mainly has a main influence on the ductility and viscosity index, the ductility is increased linearly with the increase of the DOP content, and the viscosity is increased and then decreased, so that an optimal value exists. Comprehensively, the C (DOP) level is selected to be C2. Therefore, it was determined that the preferable combinations of ZnO, PPA and DOP were added in amounts of 1.5%, 0.5% and 1.5% by weight of the base asphalt, respectively.
TABLE 3 orthogonal experiment factor horizon
TABLE 4 basic physical Properties of orthogonal experiments
TABLE 5 poor analysis of results of orthogonal experiments
K jm Is the sum of the test indexes corresponding to the j-th column factor m level, the orthogonal design of the test is 3 factor 3 level, see table 3 jm The average value of (a) can judge the excellent level of the j factor and the excellent level combination of each factor. K is j1 Namely, the sum of test indexes of j factors (three factors of A, B and C respectively represent ZnO, PPA and DOP) level 1 (table three) is shown. R is j The greater the range, the more significant the effect of the factor on the test index.
TABLE 6 analysis of variance of orthogonal test results
The equipment for penetration is a SYD-2801E1 penetration tester; the softening point is tested by adopting an HR-2806E type computer intelligent softening point tester; the ductility test adopts a low-temperature ductility extensometer produced by Beijing aerospace testing instruments, inc., and the distributed viscosity test adopts an RVDV2T rotary viscometer, and the temperature is controlled at 135 ℃.
From the basic physical properties of orthogonal experiments, when the doping amount of the nano zinc oxide is 1.5 percent of the weight of the matrix asphalt, the doping amount of the PPA is 0.5 percent of the weight of the matrix asphalt and the doping amount of the plasticizer DOP is 1.5 percent of the weight of the matrix asphalt, compared with the matrix asphalt, the needle penetration value of the modified asphalt is reduced from 7.07mm to 5.837mm, and the improvement amplitude is 17.4 percent; the softening point is increased from 52 to 58.29, and the improvement amplitude is 12.1 percent; the ductility is improved from 6.4cm to 19.89cm at 5 ℃, and the improvement range is 210.8%; the viscosity value at 135 ℃ is increased from 515 to 985.60, and the improvement range is 91.4%.
In the case of the test example 2,
five kinds of asphalts, i.e., base asphalt JZ, nano ZnO modified asphalt JN (0.5% ZnO), PPA modified asphalt JP (0.5% PPA), DOP modified asphalt JD (1.5% DOP) and ZnO/PPA/DOP composite modified asphalt JC (1.5% ZnO, 0.5% PPA, 1.5% DOP), were selected for comparison of road performance. The preparation steps of the composite modified asphalt JD are the same as those of the example 2; in JZ, JN, JP and JD, when singly doped modified asphalt JN, JP and JD is subjected to performance analysis, the optimal mixing amount is obtained, and the shearing temperature, the shearing time, the development time and the temperature in the subsequent comparison with the composite modified asphalt and the preparation step of the composite modified asphalt need to be kept consistent; the base asphalt JZ is also subjected to the same operation steps, and is used as a reference to be compared with other asphalts, and the variable of the preparation process is controlled to be consistent.
Frequency sweep test: the ultimate temperature of asphalt in summer use is about 64 ℃, so the frequency sweep is performed on an asphalt sample at 64 ℃, the storage shear modulus G' refers to the storage and release of energy during asphalt deformation, and the loss shear modulus G "reflects the energy lost in the form of heat during asphalt modulus deformation due to internal friction.
The results in fig. 4 and fig. 5 show that the G 'and G "are highest at JC, and at a frequency of 0.1Hz, G' is increased by 900% relative to JZ, and G" is increased by 425% relative to JZ, which indicates that the retention degree of the elastic component of the asphalt by the compound modifier is greatly increased, the high-temperature performance of the asphalt is obviously improved relative to that of the base asphalt, and the anti-rutting capability and the anti-fatigue capability are also obviously improved.
Low temperature rheological properties: the bending creep stiffness test is carried out on the asphalt at low temperature by using a Bending Beam Rheometer (BBR), the test temperature is selected from-12 ℃, 18 ℃ and 24 ℃, and the low-temperature crack resistance of the asphalt is jointly evaluated by using the stiffness modulus S and the creep rate m. Within specification requirements, the smaller the creep stiffness S of the asphalt, the larger the creep rate m, and the better the low temperature properties of the asphalt. As shown in FIGS. 6 to 7, the addition of the modifier DOP is obvious from the change of the numerical value on the improvement of the low-temperature performance of the asphalt, and the low-temperature flexibility and the stress relaxation performance of the asphalt become good. The JC low-temperature performance of the compound blend is greatly improved and is only second to the DOP modified asphalt.
Aging resistance:
1. aging resistance at high temperature: a Dynamic Shear Rheometer (DSR) is used for a dynamic shear rheological test, as shown in fig. 8-9, the aging index AI and the dynamic shear rheological parameter RAI of the asphalt are used as indexes for evaluating the aging resistance of the asphalt, and a smaller numerical value represents that the high-temperature aging resistance of the asphalt is better. The high-temperature aging resistance of JC can be comprehensively evaluated in five asphalt samples after short-term, ultraviolet and long-term aging, taking the data after long-term aging as an example, the AI and RAI indexes of the JC after long-term aging are minimum, and compared with the AI and RAI indexes of the JZ, the JC is reduced by 57 percent and 56 percent respectively. The composite modified asphalt JC has the best high-temperature aging resistance.
2. Aging resistance at low temperature: the Bending Beam Rheometer (BBR) was used for the bending beam rheology test, as shown in fig. 10-11; performing rheological tests on various groups of asphalt before and after short-term, ultraviolet and long-term aging at different temperatures (-12 ℃, -18 ℃, -24 ℃), and processing BBR test results in different aging modes to obtain creep rate aging index (mAI) and stiffness modulus aging index (SAI). The smaller the SAI, the larger the mAI, the better the low temperature aging resistance of the asphalt. The low-temperature aging resistance of JC comprehensively evaluated in five asphalt samples after short-term, ultraviolet and long-term aging is the best. Taking index data after ultraviolet aging as an example, after ultraviolet aging, the mAI value at-18 ℃ has a value and only the value of JC meets the specification requirement; at the temperature of minus 24 ℃, the SAI index of JC is the smallest, which indicates that the composite modified asphalt JC has the best low-temperature aging resistance.
Short term aging was tested using a SYD-0610 spin film oven. The mass of the sample asphalt is 50 +/-0.5 g, the sample asphalt is placed into a sample containing vessel, the sample containing vessel is placed into an asphalt film oven (163 +/-1 ℃), the air flow rate is 4000ml/min +/-200 ml/min, and the experimental time is 85min.
The ultraviolet curing lamp with the LED cold light source has the asphalt ultraviolet aging wavelength of 395NM and the ultraviolet intensity of 400mW/cm 2 The actual ultraviolet light intensity on the surface of the sample is 65mW/cm 2 . The test specimens were asphalt films having a thickness of 1mm, a length of 11cm and a width of 11cm after short-term aging.
The long-term aging test is a pressure aging test (PAV aging test), the test temperature is 100 ℃, the mass of the asphalt sample is 50g +/-0.5 g, the air pressure is 2.1MPa +/-0.1 MPa, and the pressure aging time is 20 +/-10 min.
The rheological test of the bending beam adopts original asphalt and asphalt after short-term, ultraviolet and long-term aging, the test load is kept at 980 nN +/-50 nN, and the test temperatures are-12, -18 ℃ and-24 ℃ respectively.
On the basis of macroscopic data analysis, microscopic scanning electron microscope tests are carried out on the asphalt, microscopic appearance observation is carried out on the asphalt, and the microscopic appearance change of the modified asphalt under different aging modes is explored. As shown in fig. 15, the nano ZnO particles are uniformly dispersed in the asphalt, and SEM observes that the surface of the modified asphalt does not have an obvious agglomeration phenomenon, but the surface is uneven and has more wrinkles; as shown in fig. 16, the PPA-modified asphalt showed floc-like surfaces. The surface of the asphalt modified by the modifier is smoother and smoother due to the addition of DOP, and does not have floccules, so that the nano zinc oxide and the PPA are more uniformly dispersed in the asphalt due to the addition of the DOP, and the agglomeration phenomenon is reduced, so that the modification effect of the modifier on the asphalt is better, as shown in figure 17.
The storage stability is mainly carried out according to a polymer modified asphalt segregation test operation method tested by T0661-2000 in test Specification for road asphalt and asphalt mixtures (JTGE 20-2011), the difference of softening points is not more than 2.5 ℃ specified in the technical Specification for road asphalt pavement construction (JTG F40-2004), and the segregation test result of JC shows that the softening point of the upper part is 57.82 ℃, the softening point of the lower part is 59.20 ℃, and the difference is 1.38 ℃, so that the storage stability meets the specification requirements.
From the results of the conventional physical test indexes, the high-temperature and low-temperature rheological property, the aging property and the fatigue property, the modified asphalt prepared by the method disclosed by the embodiment of the invention has a good comprehensive effect, and compared with the matrix asphalt and the singly-doped modified asphalt, the nano zinc oxide, PPA and plasticizer composite modified asphalt has greatly improved performance, has the road performance far exceeding that of the matrix asphalt, completely meets the requirements of pavement building materials, and has obvious economic, social and environmental protection benefits and wide application prospects.
The temperature in the preparation process of the modified asphalt is controlled below 150 ℃, while the preparation temperature of the traditional SBS composite modified asphalt is generally above 180 ℃ and even up to 200 ℃; in the experimental process of shearing modified asphalt by adopting a high-speed shearing instrument, when the temperature exceeds 175 ℃, the phenomenon that smoke gas emits is obviously observed, and more light components volatilize at high temperature; namely, the light components of the asphalt are very volatile at high temperature, and the light components in the asphalt are easy to generate oxidation reaction with oxygen in the air at high temperature, so that the prepared asphalt is very easy to generate aging phenomenon. Compared with SBS modified asphalt, the preparation temperature of the invention is reduced by 25% -30%, the influence of short-term aging of modified asphalt in the production process on the modified asphalt modification effect is greatly reduced, compared with traditional SBS modified asphalt, the energy consumption is reduced by more than 25%, because the higher the temperature is, the faster the heat dissipation is, the longer the time for heating the asphalt is needed in the actual construction by the same temperature difference, and the more the energy is consumed.
Compared with SBS modified asphalt which is used in large amount in the traffic industry at present, the modified asphalt prepared by the embodiment of the invention has the great advantages that modified asphalt with better road performance can be obtained without high preparation temperature, and after the preparation temperature is reduced, a series of beneficial effects in the aspects of environmental protection, energy and the like are brought, the problems of extremely easy volatilization of light components of the asphalt, aging of the asphalt and the like caused by high temperature are solved, the stability of the product is improved, and the phenomenon that the comprehensive road performance is greatly reduced in the production process is avoided.
In addition, the three modifiers in the embodiment of the invention are all low in price, and the engineering application capability of the invention can be greatly improved. Because the modifier is less in mixing amount and is easy to disperse, the modifier can be dispersed in the asphalt more uniformly without long-time shearing in the shearing process, so that the process is simpler than that of other modified asphalt, large and complex processing equipment is not needed in practical application, and the requirement on the equipment is lower (such as the high temperature resistance of a shearing tank, the mechanical shearing power and the like).
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention shall fall within the protection scope of the present invention.
Claims (8)
1. The preparation method of the modified asphalt is characterized in that raw materials of the modified asphalt comprise base asphalt, nano zinc oxide, polyphosphoric acid and a plasticizer, wherein the doping amount of the nano zinc oxide is 0.5-1.5 percent of the mass of the base asphalt, the doping amount of the polyphosphoric acid is 0.5-1.1 percent of the mass of the base asphalt, and the doping amount of the plasticizer is 1-2 percent of the mass of the base asphalt;
the method specifically comprises the following steps:
s1, heating and drying matrix asphalt and enough nano zinc oxide at 130-135 ℃ respectively to enable the matrix asphalt to have better fluidity; drying the water in the nano zinc oxide;
s2, taking out the matrix asphalt, uniformly heating to 145-150 ℃, and adding nano zinc oxide into the matrix asphalt, wherein the doping amount of the nano zinc oxide is 0.5-1.5% of the mass of the matrix asphalt; stirring uniformly, and shearing at high speed;
s3, adding polyphosphoric acid, wherein the mixing amount of polyphosphoric acid is 0.5-1.1 percent of the mass of the matrix asphalt, uniformly stirring, and shearing at a high speed;
s4, adding a plasticizer in a proportion of 1% -2% of the matrix asphalt, uniformly stirring, and shearing at a high speed;
and S5, putting the sheared modified asphalt into an oven at the temperature of 145-150 ℃ for development to obtain the modified asphalt.
2. The method for preparing modified asphalt according to claim 1, wherein the heating and drying time in S1 is 1-1.5 hours.
3. The method for preparing modified asphalt according to claim 1, wherein the uniform heating in S2 is specifically: and (2) putting the matrix asphalt heated in the step (S1) into a heat collection pot of a magnetic stirrer for oil bath heating, keeping the temperature at 145-150 ℃, starting a shearing machine, and stirring the matrix asphalt at the speed of 500-800r/min to uniformly heat the matrix asphalt until the internal temperature of the matrix asphalt is stable.
4. The method for preparing modified asphalt according to claim 1, wherein in S2 and S3, the shearing speed of high-speed shearing is 3000-3500r/min, the shearing temperature is 145-150 ℃, and the shearing time is 10-15min.
5. The method for preparing modified asphalt according to claim 1, wherein in S4, the shearing speed of high-speed shearing is 3000-3500r/min, the shearing temperature is 145-150 ℃, and the shearing time is 20-30min.
6. The method of claim 1, wherein in the step S4, the plasticizer is any one of dioctyl phthalate, dibutyl phthalate, tricresyl phosphate, triphenyl phosphate, and dioctyl sebacate.
7. The method for preparing the modified asphalt according to claim 1, wherein the development time in the oven in S5 is 40-60min.
8. The method for preparing the modified asphalt according to claim 1, wherein the specific surface area of the nano zinc oxide is 50-55m 2 Per g, average grain diameter of 30 +/-1 nm and purity of more than 99.5 percent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210791060.4A CN114921108B (en) | 2022-07-05 | 2022-07-05 | Modified asphalt and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210791060.4A CN114921108B (en) | 2022-07-05 | 2022-07-05 | Modified asphalt and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114921108A CN114921108A (en) | 2022-08-19 |
| CN114921108B true CN114921108B (en) | 2023-02-17 |
Family
ID=82816076
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210791060.4A Active CN114921108B (en) | 2022-07-05 | 2022-07-05 | Modified asphalt and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114921108B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115612306B (en) * | 2022-11-11 | 2023-10-17 | 长沙理工大学 | Composite modified asphalt and preparation method thereof |
| CN116178971B (en) * | 2022-11-30 | 2024-03-15 | 长沙理工大学 | Nano doped zinc oxide modified asphalt and preparation method thereof |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1339556A (en) * | 2000-08-18 | 2002-03-13 | 中国石油化工股份有限公司 | Storage stable modified asphalt and its preparing mehtod |
| CN101479344A (en) * | 2006-05-31 | 2009-07-08 | 伊诺弗斯公司 | Method for preparing an improved bitumen by addition of polyphosphoric acid and cross-linkable polymer background |
| CN101602889A (en) * | 2008-06-11 | 2009-12-16 | 中国石油化工股份有限公司 | A kind of composition that contains matrix pitch and bituminous composition and preparation method thereof |
| CN104603207A (en) * | 2012-09-12 | 2015-05-06 | 霍尼韦尔国际公司 | Bitumen compositions and methods of making |
| CN104710804A (en) * | 2015-03-17 | 2015-06-17 | 中国海洋石油总公司 | SBS (styrene butadiene styrene) modified asphalt and preparation method thereof |
| CN110272632A (en) * | 2019-07-11 | 2019-09-24 | 长安大学 | A kind of antifatigue modified pitch and preparation method thereof |
| CN110358318A (en) * | 2019-08-24 | 2019-10-22 | 深圳市交通工程试验检测中心有限公司 | A kind of high-performance road modified asphalt |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20180030276A1 (en) * | 2015-02-26 | 2018-02-01 | E. I. Du Pont De Nemours And Company | Process to modify bitumen |
-
2022
- 2022-07-05 CN CN202210791060.4A patent/CN114921108B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1339556A (en) * | 2000-08-18 | 2002-03-13 | 中国石油化工股份有限公司 | Storage stable modified asphalt and its preparing mehtod |
| CN101479344A (en) * | 2006-05-31 | 2009-07-08 | 伊诺弗斯公司 | Method for preparing an improved bitumen by addition of polyphosphoric acid and cross-linkable polymer background |
| CN101602889A (en) * | 2008-06-11 | 2009-12-16 | 中国石油化工股份有限公司 | A kind of composition that contains matrix pitch and bituminous composition and preparation method thereof |
| CN104603207A (en) * | 2012-09-12 | 2015-05-06 | 霍尼韦尔国际公司 | Bitumen compositions and methods of making |
| CN104710804A (en) * | 2015-03-17 | 2015-06-17 | 中国海洋石油总公司 | SBS (styrene butadiene styrene) modified asphalt and preparation method thereof |
| CN110272632A (en) * | 2019-07-11 | 2019-09-24 | 长安大学 | A kind of antifatigue modified pitch and preparation method thereof |
| CN110358318A (en) * | 2019-08-24 | 2019-10-22 | 深圳市交通工程试验检测中心有限公司 | A kind of high-performance road modified asphalt |
Non-Patent Citations (2)
| Title |
|---|
| Polyphosphoric acid and plasticizer modified asphalt: Rheological properties and modification mechanism;Ruimeng Song等;《Construction and Building Materials》;20211012;第309卷;第1-12页 * |
| 纳米氧化锌改性沥青及其抗老化性能研究;张明详;《中国优秀硕士学位论文全文数据库工程科技Ⅱ辑》;20160215(第2期);第B020-199页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114921108A (en) | 2022-08-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN114921108B (en) | Modified asphalt and preparation method thereof | |
| Zhang et al. | Evaluation of aging behaviors of asphalt with different thermochromic powders | |
| Chen et al. | The performance of hot-recycling asphalt binder containing crumb rubber modified asphalt based on physiochemical and rheological measurements | |
| Bonemazzi et al. | Shifting the bitumen structure from sol to gel | |
| Gu et al. | Study on rheology and microstructure of phenolic resin cross-linked nonionic polyacrylamide (NPAM) gel for profile control and water shutoff treatments | |
| CN105754356B (en) | A kind of bitumen regenerant and its preparation method and application | |
| CN108980622B (en) | Nano composite pour point depressant, and preparation method and application thereof | |
| Ren et al. | Modification mechanism and enhanced low-temperature performance of asphalt mixtures with graphene-modified phase-change microcapsules | |
| Wang et al. | Properties and mechanism of SBS/crumb rubber composite high viscosity modified asphalt | |
| Meng et al. | Study on aging resistance and micro characteristics of bio-asphalt/TLA composite modified asphalt binder | |
| CN112679898B (en) | Vinyl chloride-acrylate copolymer modified water-based asphalt and preparation method thereof | |
| Peng et al. | Laboratory evaluation of different bio-oil recycled aged asphalts: Conventional performances and microscopic characteristics | |
| He et al. | Preparation and performance assessment of asphalt emulsion modified by the fabricated SBS latex | |
| Yeşilçiçek et al. | Characterization and rheological properties of asphalt binder with a novel tall oil-based boron additive to enhance asphalt performance | |
| Cui et al. | Preparation of chlorinated poly (propylene carbonate) and its effects on the mechanical properties of poly (propylene carbonate)/starch blends as a compatibilizer | |
| CN111087828B (en) | Sasobit warm mix asphalt and preparation method thereof | |
| Zhou et al. | Strong thickening performance and mechanism of supramolecular system constructed by β-cyclodextrin polymer included adamantane polymer | |
| CN113248809A (en) | Plasticizing modified warm-mix agent and warm-mix asphalt preparation method | |
| CN112226095A (en) | Preparation method of low-cost anti-segregation aging-resistant modified asphalt | |
| CN116333508A (en) | Stable star-line blending SBS modified asphalt based on molecular lubrication and preparation method thereof | |
| Zhang et al. | Improved properties of weathered coal and SBR/weathered coal compound modified asphalt | |
| CN115044099B (en) | Two-dimensional asphalt warm mix agent suitable for ultralow-temperature construction of hot mix asphalt mixture, warm mix asphalt and preparation method thereof | |
| CN116102894B (en) | Organogel modified asphalt and preparation method thereof | |
| CN115304303B (en) | Method for delaying asphalt aging by utilizing porous calcium carbonate microsphere slow-release regenerant | |
| Zhang et al. | Research on Vegetable Oil Based Rejuvenating Agent and Properties of Recycled Asphalt |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |